Production of rosin and turpentine



Filed Nov. 26,' 1941 FIG. I

' INVENTOR Jesse Red ATTORNEYS Patented Nov. 28, 1944 UNITED "STATE sPATENT OFFICE.

PRODUCTION OF ROSIN AND TUR-PENTINE Jesse 0. Reed, Washington, D. 0.,assignor to Claude R.- Wickard, as Secretary of Agriculture of theUnited States of America, and his successors in office ApplicationNovember 26, 1941, Serial No. 420,540-

1 Claim.

(Granted under the act .of March 3, 1883, as amended April 30, 1928; 3700. G. 757) steam or water wasadmitted to carryover the turpentine at lowtemperatures. At approximately 210 F. the turpentine begins to distillfrom the oleoresin, and the distillation is usually completed at about315 F., the material remaining in the vessel being rosin. By thisprocess, ap-' proximately two parts of water, as steam, are required todistill three parts of turpentine initially. As the distillationcontinues, more and more steam is required until at the end about 19parts of water, as steam, are required to distill one part ofturpentine. The use of the batch method, therefore, requires largequantities of heat and, furthermore, as the distillation proceeds, thecomposition of the turpentine changes, due to the fact that theconditions of distillation are not constant throughout with respect totemperature and the composition of the materials in the still.

The general object of this invention is the provision of a process andapparatus for manufacturing turpentine and rosin from oleoresin whichwill result in the production of turpentine and rosin having uniformcompositions and which will not require excessive amounts of steam todistill the turpentine thereby reducing the amount of required heat.

A further object of this invention is to provide a method of the typementioned b virtue of which the materials are not subjected to prolongedheating, as in the batch process. Such prolonged heating adverselyinfluences the grade of the rosin produced.

To accomplish theseobjectives, I have provided means whereby theturpentine can be distilled in a continuous process, rather than inbatches, and such that the conditions of distillation can be maintainedsubstantially constant without prolonged heating, resulting in a uniformcomposition of both turpentine and rosin.

In the accompanying drawing, there is illustrated a'preferred embodimentof an apparatus for carrying-out the process of my invention andconsidered together with the following description a full understandingof my invention may be had by those skilled in the art.

In the drawing referred to:

Figure 1 is a diagrammatic elevational view of a preferred embodiment ofthe apparatus of my invention, partly in section.

Figure 2 is a section along the line 2-2 of Figure 1;

Figure 3 is a section along the line 3-3 of A Figure 1.

Referring with more particularity to the drawmg in which like numeralsdesignate like parts. the apparatus illustrated comprises a verticalpipe I I into the bottom of which filtered oleoresin is fed by a pumpl2. As the oleoresin proceeds through the pipe II, it is heatedexternally by steam admitted through an inlet I3 of a steam jacket M toa temperature exceeding the boiling point of the oleoresin, about 210 F.The outlet of the steam 'jacket I4 is designated by the numeral l5.Leaving the'upper end of the pipe H, the oleoresin is forced throughpipes l6 and I! to a liquid spray nozzle [8 in the upper part of achamber I9. Th upper endof the chamberl9, above the nozzle l8,contains'packing 20, such as Raschig rings, and a vapor outlet.

2| at the top is connected to a condenser (not shown) by means of a pipe22. The lower end of chamber 19 has an outlet23 connected to the top ofa column 24. The hot oleoresin passing through the nozzle I8 is sprayeddownwardly in finely divided form into the chamber IS. A pipe 25 isconnected at the bottom of the column 24 is sprayed downward from thenozzle [8 and vaporizes a large portion of the turpentine in the spray.The turpentine vapors then pass upward with the steam into th upper endof chamber l9 and out through the outlet 2! and pipe-22 into thecondenser fronr whence the turpentine is separated from the condensateand recovered. The baflle efiect of the packing 20 prevents nonvolatilematerials from passing into'the condenser through the pipe 22; Theremaining part of the oleoresin fallsunder the action of gravity isvaporized and forced upward through the chamber I9 and out through theoutlet 2|, leaving the non-volatile material to collect at the bottom ofcolumn 24 and flow into the bottom of a vertical pipe 32 through aconnecting pipe 33, the flow being controlled by the valve 34 insaidpipe 33. The pipe 32 is also provided with a steam jacket 35 having asteam inlet 36 and outlet 31.

The material entering the pipe 32 at the bottom is substantially free ofturpentine and consists essentially of rosin and water. If the rosinwere recovered'at this point, the water contained therein would uponcooling of therosin cause it to become opaque, which is undesirable.Such rosin is ordinarily unmarketable. Consequently, in order to obtaina clear marketable rosin, it is necessary to free the material of thiswater. This is accomplished in the subsequent steps of the process. Thewater-containing rosin as it flows upward through the pipe 32 is kept inrising oif the bottom of the chamber 52, from which function to retardthe flow of the rosin so as to permit it to absorb more heat as itpasses through the column and, at the same time, placing it into contactwith the hottest part of the column, leaving sufiic'ient opening for theupward passage of vapors through the column. The use of such screens,however, is not indispensable, and other satisfactory means may be used.For example, baffles, such as the ones shown in column 24,:may beemployed to impart a whirlingmotion. Such baiiles may be used either insubstitution of the conical screens 49 or in conjunction with them.

The anhydrous and turpentine-free rosin collects at the bottom of thecolumn 45. From this point the flow is controlled by a valve 50 fromwhich the rosin passes through a pipe 5| into the bottom of a chamber52. The chamber 52 is provided with a steam jacket 53 having an inlet 54and outlet 55 to keep the rosin in a fiuid state. The upper end of thechamber 52 is provided with a vent 56 so that'any free water, which maybe carried into the chamber 52, will be immediately distilled off by theexcess heat of the rosin, which at this point may be as high as 330 F.The rosin collecting in the chamber 52 is discharged through a pipe 51which is disposed through the side of the chamber 52, the

intake opening 58 extending downward in the direction opposite the vent56.- To prevent steam;

entering the inlet 58', abattle 53 is provided helow the outlet 58.Rising steam passes around a fluid state by heat from the steam jacket35.

This heat also vaporizes the Water in the mass and any traces ofturpentine which might remain. These vapors force the rosin upward inthe pipe 32 through a connecting pipe 38 at the top, and thence througha downwardly extending pipe 39 which terminates in the upper part.

of an expansion chamber 40, similar to the chamber IS. The lower end ofthe pipe 39 is also provided witha liquid spray nozzle 4|, similar tothe nozzle 8, and at the top of the chamber 40 a vapor outlet 42 issimilarly provided which is connected by a pipe 43 to a second condenser(not shown). The upper part of the chamber '40 is likewise provided withpacking material 44;

like that in the'chamber I9- and for the same purpose. Asthe rosinpasses through the pipes 33 and 39, it 'is. forced through the spraynozzle 4|. The steam associated with the rosin aid any turpentine vaporsformed are immediately released, rise and pass into the second condenserthrough the outlet 42 and pipe 43. The bottom of the chamber 40 isconnected to the top of a column 45 which is kept hot by a steam jacket'45 having an inlet 41 and outlet 48. The rosin falling from the nozzle4| collects in the bottom of the chamber 40 and passes downward throughthe column 45. Should any turpentine or moisture remain in the rosin asit proceeds down through the column 45, it is vaporized'by heat from thesteam in the jacket 45. 4 In order to increase the efiectiveness of thisaction, it is preferred to have the material flowing downward in thecolumn 45 as close to the steam jacket as possible. To accomplish this,conical shaped screens 48 of wire, rial, are secured at intervals in'thecolumn' 45 said packing material, said nected to one end of saidconduit, said chamber having an outlet at the top,

the baflle 59 and by-passes the outlet 58, from whence it proceeds outthrough the vent 56 while the fluid rosin is forced into the inlet 58and through the pipe 51, from whence it is recovered in an anhydrouscondition ready for marketing.

Having thus described my invention, I claim:

A distillation apparatus comprising a conduit, a chamber, packingmaterial at the topof said chamber, a spray nozzle in nozzle being conacolumn having a free vertical space and having its upper end connectedto the bottom of said chamber, means for rotationally introducing steaminto the bottom of said column, means for causing steam rising in saidcolumn to whirl, a second conduit having one end connected to the bottomof said column, a second chamber, packin material at the top of saidsecond chamber, a nozzle in said second chamber below the packingmaterial therein, said second chamber having an outlet at the top, saidnozzle being connected tothe other end of said second conduit, asecondcol- -umn having a free vertical space and having its or any othersuitable mateupper end connected to the bottom of said second chamber,baflies in said second column foriorcing descending material outwardly,a receptacle, the bottom of said receptacle being connected to thebottom of said second column, said receptacle having a vent at the topand a down- 'wardly facing outlet below said vent, and a .bame belowsaid outlet to by-pass vaporsaroundsaid outlet, 'and means forexternally heating said conduits, columns, and said receptacle.

JESSE O. REED.

said chamber below

